SUMMARY

This experiment is about the determination of Iron (Fe) by using Atomic Absorption
Spectroscopy (AAS). AAS is the elemental analysis technique commonly used for detecting
metals and metalloids in samples. The experiment begin with preparing the 100 ppm of
copper (Cu) standard dilution with the addition of 1% (v/v) of concentrated nitric acid (1% =
1 ml). Then, a serial dilution of 0.5 ppm, 1.0 ppm, 1.5 ppm, 2.0 ppm, 2.5 ppm and 4.0 ppm
(Cu) standard solution was prepared. Then, duplicate 1 mL of 0.2M of nitric acid mixed with
filtered water until it becomes 100 mL solution. The prepared samples will be put through the
AAS for reading. The readings will show the amount of Fe present in each of the sample
prepared. Calibration curve will be obtained by the readings which show the relationship
between the Absorbance (Abs) and the Concentration (ppm). Absorbance readings for
unknown samples 1 and 2 were obtained which were 0.8045 ppm and 1.700 ppm
respectively. Meanwhile for concentrations 0.5,1.0, 1.5, 2.0, 2.5 and 4.0 ppm, absorbance
readings of 0.019, 0.046, 0.106, 0.110, 0.136 and 0.235 nm were obtained in order. It can be
observed that the values obtained from the graph plotted and the theoretical graph was
similar. Therefore, based on the results, the objectives of this experiment were achieved.

INTRODUCTION

Atomic Absorption Spectroscopy is an elemental analysis technique that is frequently

used in the environmental, metal, food, pharmaceutical, and chemical sectors to analyse
materials.Atomic Absorption Spectrometry (AAS) uses distinctive wavelengths of
electromagnetic radiation from a light source to identify components in liquid or solid
samples. Individual elements absorb wavelengths in different ways, and the absorbances of
these elements are compared to standards.Because of their specificity, sensitivity, accuracy,
simplicity, and cheap cost per analysis, AAS methods are chosen in the clinical
laboratory.(Smith, 2015). In fact, AAS takes use of the various wavelengths of light that are
absorbed by certain atoms. (Atomic Absorption Spectrometry (AAS) InformationThermo
Fisher Scientific - MY, 2021)
 A solution containing the analyte is injected into a flame in AAS. The flame turns
samples into excitable free ground state atoms. A lamp generating light with a wavelength
specific to the atoms is passed through the flame, and the electrons in the atoms are activated
when the light energy is absorbed.

Figure 1: Schematic Diagram of AAS

The Beer Lambert law outlines the link between element concentration and light
absorption. The amount of light absorbed is proportional to the number of atoms in the flame
that have been stimulated from their ground state, according to the law.(Atomic Absorption
Spectroscopy, How Does AAS Work, AAS FAQs. Agilent, 2021)

The Beer Lambert Law defines the relationship between the concentration and
absorption of an absorbing species.
A= bc

Where:
A: is the absorbance (Abs). Abs is measured by the AAS.
: is the wavelength at which absorption is observed for the element of interest?
b: is the pathlength. For flame AAS, this is typically the path length through the flame
(alongthe burner) and is fixed for all measurements.
c: is the determined concentration of the element.

The main goal of this experiment is to use Atomic Absorption Spectroscopy (AAS) to
determine the amount of copper (Cu). The experiment begin with preparing the 100 ppm of
copper (Cu) standard dilution with the addition of 1% (v/v) of concentrated nitric acid (1% =
1 ml). Then, a serial dilution of 0.5 ppm, 1.0 ppm, 1.5 ppm, 2.0 ppm, 2.5 ppm and 4.0 ppm
(Cu) standard solution was prepared. The prepared samples will be put through the AAS for
reading. The readings will show the amount of Fe present in each of the sample prepared.
Calibration curve will be obtained by the readings which show the relationship between the
Absorbance (Abs) and the Concentration (ppm).

OBJECTIVES

a) To optimize the burner system by flame AAS using standard solution.

b) To check the performance (sensitivity) of the atomic absorption spectroscopy using
standard solutions.
c) To prepare a serial dilution and generate a standard calibration curve
d) To determine the amount of copper (Cu) in the unknown sample

Materials

1. 1000 ppm of Copper (Cu) stock solution

2. Concentrated nitric acid (69%),

3. Deionized water

4. Sample containing unknown concentration of copper

Equipment

1. Beaker 250 mL

2. Pipette 5 ml & 10 mL

3. Volumetric Flask 100 mL

4. Rubber Bulb

5. Glass Dropper
Procedure

A.Preparation of100ppmofcopperstandardsolution

1% (v/v) of concentrated nitric

10 mL of 1000 ppm copper stock acid (1% = 1 ml) was added into
solution was pipetted into a 100 the volumetric flask and marked
ml volumetric flask. up to the mark level with
deionized water.

B. Preparation of copper standard solutions

The exact volume of 100 ppm of copper

standard solution (from part A) was pipetted to
prepare a series of standard solution with
concentrations of 0.5 ppm, 1.0 ppm, 1.5 ppm,
2.0 ppm, 2.5 ppm and 4.0 ppm.

[The volume was calculated by using : M1V1 =

M2V2]

1% v/v of concentrated nitric acid was added to

each of the standard solution and mark up to the
mark level with deionized water.
C. Operating the AAS

Optimizing the Burner system

A blank solution was

prepared - pipette 1% v/v
of concentrated nitric acid The known standard solutions
was pipetted into 100 ml was aspirated using 2 ppm
volumetric flask and and 4 ppm.
deionized water was added
until the mark level.

The burner position was

adjusted using the horizontal
The absorbance of blank
adjustment knob and the
solution was checked again
nebulizer adjustment nut until
and it should be zero.
a maximum absorbance was
displayed on the screen.
Formula

The formula used for the preparation of the serial dilution of Cu standard solution is:

RESULT

1. Analysis of data

A) Comparison characteristics concentration value ( 2 ppm ) : 0.073 mg/L

B) Measured characteristics concentration value ( 2 ppm ) : 0.077 mg/L

C) Comparison characteristics concentration value ( 4 ppm ) : 0.073 mg/L

D) Measured characteristics concentration value ( 4 ppm ) : 0.077 mg/L

2. Checking performance of the instruments

Calculate characteristics concentration for Standard solution 2 ppm & 4 ppm using equation
below:

a) Characteristics Conc. Value = (0.0044 × 2 ppm) ÷ 0.110 nm

= 0.080

b) Characteristics Conc. Value = ( 0.0044 × 4 ppm ) ÷ 0.236 nm

= 0.0746
 3. Creating a Standard Calibration Curve
Record the absorbance readings and the unknown concentration in the table below:

No. Concentration of Absorbance

Standard Solution (ppm) (nm)
1 0.5 0.019
2 1.0 0.046
3 1.5 0.106
4 2.0 0.110
5 2.5 0.136
6 4.0 0.235
7 Unknown 1 0.8045
8 Unknown 2 1.700

Concentration Vs Absorbance
0.25 0.235

0.2
Absorbance (nm)

0.15 0.136

0.106 0.11

0.1

0.046
0.05
0.019

0
0 0.5 1 1.5 2 2.5 3 3.5 4 4.5
Concentration (ppm)
DISCUSSION

In this experiment, the main purpose atomic absorption spectroscopy is to determine

the concentration of copper in tap water by using AAS. This method is commonly used by
detecting the heavy metals in sample. The technique of atomic absorption spectroscopy, or
AAS, is used to determine the amounts of metallic elements in various materials.
Electromagnetic wavelengths from a light source are used as an analytical tool. These
wavelengths will be absorbed differently by different elements Invalid source specified..

In this experiment tap water were already done by the technician. After the series of
standard dilution (0.5 ppm, 1.0 ppm, 1.5 ppm, 2.0 ppm, 2.5 ppm and 4.0 ppm) were prepared
by using the equation, the nitric acid were added 1% into dilution and were filled up with
distilled water. The instrument was calibrated using several solutions of known concentration
and were aspirated first with two dilution of concentration which is 2 ppm and 4 ppm. The
results of absorbance turned out was 0.110 nm for 2 ppm concentration and 0.235 nm for 4
ppm concentration.

The standard solution also have been done by using two samples unknown which is
unknown 1 and unknown 2 and the results were turned out is 0.8045 nm for concentration
unknown 1 and 1.700 nm for concentration unknown 2. Absorbance measurements were
obtained from the data for samples 1 to 5 ( concentration 0.5 ppm, 1.0 ppm, 1.5 ppm, 2.0
ppm, 2.5 ppm and 4 ppm) is 0.019 nm, 0.046 nm, 0.106 nm, 0.110 nm, 0.136 nm and 0.235
nm.

The absorbance of each known solutions was measured and the calibration curve of
Copper concentration against absorbance were plotted in the graft. The graft shown that all
the concentration were plotted in the linear line while for the concentration of 1.5 ppm was a
bit more highly than the others absorbance that make the results not achieve the optimization
that supposedly obtained. This can be equated to the objective about the instruments
characteristics which is it is sensitive to slight changes in flame conditions. In other word,
while making the preparation standard solution for the concentration it may be slightly
mistakes while making it. The other objectives were achieved which is prepared a serial
dilution and generate the calibration curve, determine the amount of copper in the unknown
sample and optimize the burner system by flame AAS using standard solution.
CONCLUSION

The use of Atomic Absorption Spectroscopy is important to this investigation (AAS). The
outcomes were displayed on a printed page. The dilution equation was used to do
calculations, and serial dilutions were made to serve as a standard and to undergo analysis in
order to obtain a calibration curve. A graph of absorbance against concentration (ppm) was
plotted based on the data, and a comparison was done with the theoretical graph based on the
results. For unknown 1, the theoretical graph yielded a reading of 0.8045, while the displayed
graph yielded a reading of 0.8045. In the case of unknown 2, the theoretical graph yielded a
reading of 0.1700, but the plotted graph yielded a result of 1.700. The results derived from
the graph depicted and the theoretical graph were similar, as can be seen.Therefore, based on
the results, the objectives of this experiment were achieved.

RECOMMENDATION

Reading the lab manual ahead of time will provide you a quick overview of how the
experiment works and will greatly lessen the chances of making mistakes. The volumetric
flasks used in the experiment must be thoroughly cleaned to ensure that the sample does not
mix with other samples. Furthermore, the material provided for experimenters' use in
conducting the experiment must be free of contamination. It is highly recommended that you
get assistance from the professional. Furthermore, because the serial dilution procedure is a
permanent operation, the addition of distilled water must reach the mark and should not
exceed the limit.As a result, executing the serial dilution with a dropper will avoid this error
from occurring and will aid in getting maximum precision and accuracy in results. Aside
from that, there's a chance that parallax error will occur during the experiment. As a result,
one of the best strategies to avoid errors is to manage the serial dilution on a flat and sturdy
surface.
APPENDIX